CN1793162A - Tech. for producing dioscorea sapogenin - Google Patents
Tech. for producing dioscorea sapogenin Download PDFInfo
- Publication number
- CN1793162A CN1793162A CN 200510022745 CN200510022745A CN1793162A CN 1793162 A CN1793162 A CN 1793162A CN 200510022745 CN200510022745 CN 200510022745 CN 200510022745 A CN200510022745 A CN 200510022745A CN 1793162 A CN1793162 A CN 1793162A
- Authority
- CN
- China
- Prior art keywords
- sapogenin
- production
- diosgenin
- technology
- new process
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Saccharide Compounds (AREA)
- Steroid Compounds (AREA)
Abstract
The invention relates to a new manufacture technology for dioscin that uses 2-3 years growth ginger or japanese yam root crown as raw material. The process includes the following steps: raw material, smashing, super sound distillation, rectification, dissolving and purifying, rectification, saponin, cracking, rectification, dioscin. The invention is low cost, low raw material consumption, high quality, no pollution.
Description
One, technical field
The present invention relates to a kind of new process of production of diosgenin.
Two, background technology
The saponin of extracting from yellow ginger or Ningpo Yam Rhizome (being dioscin) is the precursor of steroid hormone class medicine, accounts for 70% in the raw material of synthesizing steroid medicine.In world's medicine family, the steroid hormone medicine is the second largest class medicine that is only second to antibiotic.The steroid hormone types of drugs of produced worldwide reaches 292 kinds more than at present according to statistics.The steroid hormone medicine has very strong anti-infective, antianaphylaxis, antiviral and antishock pharmacological action, clinically at home and abroad pharmaceutically widely uses.So far diosgenin is still the synthetic optimal raw material of this class medicine.
Since the nineties, world market steroid hormone sales amount of medicine every year increases progressively about with 4.3%-8%, and is synchronous therewith, the whole world to the demand of saponin also to be not less than 6% speed increment.According to external medicine scholarly forecast: in following 20 years, the steroid hormone medicine company still is remarkable rising situation, and its demand is increasing, and Europe will be with annual 5.2%, and the U.S. is with 4.4%, and the Asia is with 7.7%, and Africa, South America are with 13% surge.
The traditional processing technology of diosgenin is:
1, the fermentation extraction sapogenin that combines with acid hydrolysis
Fresh ginger cleaning → pulverizing → fermentation → acidolysis → washing neutrality → drying → gasoline extraction → sapogenin
2, the fermentation method extraction sapogenin that combines with enzymolysis
Fresh ginger cleaning → pulverizing → fermentation → enzymolysis → drying → gasoline extraction → sapogenin
Domestic main employing at present be that fermentation is extracted sapogenin with acid-hydrolysis method.
It is the technical big breakthrough that do not have that saponin produces the problem that exists, and saponin produces and prolongs the production technique of extracting with spontaneous fermentation, dilute hydrochloric acid hydrolysis, industrial naptha always, and gained saponin quality is lower.Traditional technology is keeping effective constituent, removes the invalid components aspect, exists that energy consumption is big, material consumption is big, loss of effective components is big, impurity is many, efficient is low, the cycle is long, operation is many, the not high shortcoming of extraction yield.Concrete manifestation is as follows:
1, fermentation period is long, easily goes mouldy, and it is not thorough to ferment.
When 2, being washed to neutrality, water loss is big, pollutes greatly, and causes sapogenin to run off.
3, finished product per ton consumes acid 15-18 ton the most.
4, finished product loss gasoline 5-6 ton per ton.
Three, summary of the invention
The purpose of this invention is to provide a kind of technology advanced person, less investment, raw material consumption is low, quality product is high, product are of fine quality, the new process of production of with short production cycle, free of contamination a kind of diosgenin.
The object of the present invention is achieved like this:
1, choosing 2-3 gives birth to yellow ginger or Ningpo Yam Rhizome collar (water ratio is less than 7%) and carries out coarse reduction and make its granularity reach 2-3mm
3, be crushed to 5-10um with supper micron mill again;
2, in solid particles, cooperate reverse-flow ultrasonic circulating extracting machine to make cell wall breaking with 90-95% ethanol or methyl alcohol and handle, filter and collect vat liquor, remove filter residue.To separate pure liquid and do concentrated the distillation: A, alcohol solvent rectifying are reclaimed and are reused, and ethanol concentrated solution adding skim soln evaporated under reduced pressure gets total saponin; B, ethanol are concentrated into flocks and separate out, and after cold washing with alcohol flocks degreasing, 60-90 ℃ of heat drying gets yellow saponaceous solid.
3, add the immersion of purifying waste water in the saponaceous solid of yellow, volume is 10 times of solid, is lower than 95 ℃ of heating to accelerate immersion speed, and filtrate liquid after 30 minutes is with insolubles 60-160 ℃ drying.
4, dry thing adds 90-95% ethanol or methyl alcohol and is heated to dissolving fully; The canescence insoluble solids is separated out in cooling, and the micro-pore-film filtration reject is separated out impurity; 85-120 ℃ of heating concentrates reclaims pure liquid, and alcoholic solution concentrates to be cooled to separates out flocks fully, leaches pure liquid; 60-160 ℃ of drying separated out flocks and got saponin.
5, refining saponin or total saponin heating for dissolving be in the 15-35% hydrochloric acid soln, and heating pyrolyze 4 hours becomes clear to liquid, hydrochloric acid solution and flocculent precipitate, leach acid solution.
6, neutralize with 1% yellow soda ash in flocculent precipitate, be washed to neutrality, cryodrying gets the crude product sapogenin.
7, be aided with and be lower than 80 ℃ and be heated to after crude product sapogenin solid substance dissolves fully by adding ethanol in the crude product sapogenin, stop heating; Add activated carbon powder, pure liquid micro-pore-film filtration.
8, reclaim alcoholic solution, 60-160 ℃ of cryodrying gets the elaboration sapogenin, or directly gets the elaboration sapogenin at 80 ℃ of evaporating solvents.
The new technology that is applied in this technology: (1) superfine communication technique; (2) high-shear technology; (3) reverse-flow ultrasonic circulating extractive technique; (4) screw settling isolation technique; (5) adopt the reciprocal lixiviate of chemical solvents; (6) membrane filtration technology; (7) electrodialysis technology.
Ultrasonic wave interpolation organic solvent is made the broken wall treatment described in the broken wall treatment in this technology needs organic solvent cooperate reverse-flow ultrasonic circulating extracting machine to use;
In this technology, organic solvent is return-flow type and reuses.
Illustrate: 1 total saponin can directly add acid cleavage, and deficiency is to carry a large amount of impurity secretly.Reduce the quality of sapogenin.
2 crude product saponins can adopt electrodialysis to separate glucoside unit with electrolysis tech.
The new technology that the present invention is applied to is:
(1), superfine communication technique
Particle diameter is a micro powder granule less than the powder granule of 10um, utilizes modern advanced mechanical disintegration technology that raw material is broken for the technology of micro powder granule, is called ultrafine powder or superfine communication technique.
Adopt micronizing equipment powder particle diameter can be brought up to 5um-10um, plant powder can reach 95% broken wall level.The micronizing Controllable Temperature is built in middle temperature, low temperature, very low temperature, and the medicinal material that contains different physico-chemical property compositions all can adopt.And this kind new technology is suitable for inhomogeneous medicinal material.Ultra-micro powder can make that effective constituent is able to abundant reservation in the crude drug, and the stripping of effective constituent is rapider, it is faster, more abundant to discharge, and absorption process is more direct, quick in the body, and utilization ratio of drug improves greatly.
(2), high-shear technology
Material in entering the working chamber of high-shear emulsion machine after, moment bears hundreds of thousands of time and shears, produced simultaneously turbulent flow makes material be subjected to more powerful fluid power and shears.Because the comprehensive action of some kinds of Cracking Mechanisms such as shearing, bump, extruding, grinding makes material just fully reach the purpose of dispersion, mixing, emulsification, homogeneous, fragmentation in the extremely short time, makes the target product complete processing more superior, quality product is more stable.
(3), circulating ultrasonic extractive technique
Ultrasonic wave mainly contains the effect aspect three in the supersound extraction process.
1., ultrasonic wave is propagated in medium and can be made the medium particle enter the diffusion of vibrational state reinforcement solute, mass transfer, i.e. ultra sonic machinery mechanism in its communication space.
2., ultrasonic wave its energy in medium particle communication process constantly absorbs by the medium particle and becomes heat energy, causes medium particle temperature to raise, i.e. ultrasonic wave calorifics mechanism.
3., simultaneously the ultrasonic wave of working as macro-energy acts on the extraction medium, and when vibration was in rarefaction state, medium was torn into many little holes, and these little holes are instantaneous promptly closed, produce the transient pressure up to several kilo-atmospheric pressures when closed, i.e. cavitation phenomenon.Micro-bubble in ultrasonic field in the liquid at first experiences the vibration and the process of growth of bubble, both stable cavitation; Be compression and collapse process, the both transient cavitation of bubble then.The enormous pressure that the explosion of micro-bubble produces in the cavitation causes be broken thing cell walls and whole organism to break, and whole rupture process finishes in moment, and the oscillating action that produces of ultrasonic wave has been strengthened release, diffusion and the dissolving of intracellular organic matter simultaneously.
The ultrasonic disruption process is a physical process, does not have chemical reaction in the leaching process, is remained unchanged by the biologically active substance of lixiviate, can greatly improve extraction efficiency.Ultrasonic wave is made its effect of time spent and is not only depended on hyperacoustic intensity and frequency, and with the structure function of the thing that is broken certain relation is arranged.Bubble size is not single in the medium owing to extract, but has a distribution range, so ultrasonic frequency should have certain range, a bandwidth is arranged promptly.Through systematic study to ultrasound-enhanced extraction property, according to biochemical engineering theory and method, the material circulation has been proposed, the ultrasonic field stationary distribution, simulate between material and the ultrasonic field mobile, thereby improved the utilization ratio of ultrasonic field to greatest extent, when having solved static material supersound extraction simultaneously sphere of action limited, extract the limited problem of raw material, circulate appropriate design with ultrasonic field by employing, greatly increased the material treatment capacity of ultrasonic field.
The ultimate principle of ultrasound assisted extraction technique mainly is that the leaching that utilizes cavitation effect of ultrasonic waves to quicken effective ingredients in plant is extracted, hyperacoustic in addition second-order effect, as mechanical vibration, emulsification, spread, smash, chemical effect etc. can quicken also that desire extracts that the diffusion of composition discharges and fully and solvent, be beneficial to extraction.Compare with conventional extraction method, have extraction time short, productive rate is high, need not advantages such as heating.Ultrasound assisted extraction technique can be avoided the destruction of High Temperature High Pressure to effective constituent.
(4), screw settling isolation technique
Screw settling centrifuge is to utilize the density difference of sedimentation principle with solid, liquid phase in the suspension, the centrifuge field that is produced at rotary drum internal cause high speed rotating makes solid phase fall to rotatory drum wall rapidly, thereby make solid, liquid two-phase be separated into sediment and parting liquid, be applicable to volumetric concentration≤40%, solid phase density greater than density of liquid phase, have the separation of the suspension of certain flowability; Have separating factor height, work continuously, throughput is big, adaptability is good characteristics, and can clarify various materials, dehydration, progressive operation.
(5), adopt the reciprocal lixiviate of chemical solvents
The target solute of solid particulate inside can cause solubleness to reduce in solvent because of solubleness is saturated after the supersound process, and the part solute is trapped in the particle; Solid particles after separating is done the secondary lixiviate make solute stripping more completely, improve extraction yield.And the solubleness of starch in solvent and small, can omit the starch separating technology, shortened extraction time, simplified abstraction process, improved the purity of product.
(6), membrane filtration technology
The separating mechanism of many empty films mainly is sieving action; The separating mechanism of dense film generally is a dissolving-diffusion.The former is mainly used in ultrafiltration, micro-filtration, dialysis etc.; The latter is mainly used in reverse osmosis, gas delivery, infiltration gasification etc.The liquid film separating mechanism is that dissolving-diffusion is transmitted with promotion.Improve the purity of purifies and separates
(7), electrodialysis technology
Dialysis method is to utilize small-molecule substance can pass through semi-permeable membranes in solution, and macromolecular substance can not reach isolating a kind of purification process by the character of semi-permeable membranes.Be usually used in the bigger material of separation and purification molecular mass, to remove impurity such as inorganic salt, monose, disaccharide.Whether success is very big with the gauge relationship of dialysis membrane in dialysis, need select according to the particular case of desiring separated component.Dialysis membrane is divided into animality film, collodion membrane, parchment film (template film), protein glued membrane, cellophane film etc.Need in the dialysis procedure often to change clear water, the concentration difference of the inside and outside solution of dialysis membrane is strengthened, to accelerate dialysis speed, suitably heating in case of necessity, and stirred.Soak molten solvent two ends and place two electrodes in order to accelerate the dialysis speed dialysis membrane of being everlasting, feed direct supply, can make the dialysis speed of charged ion increase more than 10 times.
Novel process and traditional technology cost contrast (relatively) with finished product per ton:
| Project | Novel process | Old technology |
| Treatment time | 1-2 hour | Fermented 48-72 hour |
| Extraction time | 8-24 hour | 5-6 days |
| Solvent loss | Solvent is roughly equal to 10,000 yuan of Renminbi for 2 tons | 120 #Gasoline is roughly equal to 40,000 yuan of Renminbi for 6 tons |
| Acid consumption | 1 ton | 15 tons-18 tons |
| Pollute | 2 tons of the waste liquid less thaies that produces when 1, cleaning can be recycled after the neutralization.2, acid hydrolysis solution can be collected, and market price is with 15 yuan of/ton recovery. | 500-1000 ton waste water (starch-containing, strong acid and wood fibre) can't reclaim |
| Current consumption | 2000KW | 2000KW |
| Raw material consumption | 40 tons (dry weight) | 130 tons (weight in wet base) |
| Technology | Automatically with individual can the switching arbitrarily of semi-automatic knot mutually, omnidistance flowing water is worked continuously, and extracts precision and rate of recovery height.Operator are few, save cost. | Artificial Control, batch operation.Low operator are many for yield. |
| Technology is used | Micronizing, high-shear technology, ultrasonic wave, screw settling isolation technique, membrane filtration, electrodialysis technology | Acid hydrolysis, fermentation |
Four, description of drawings
Accompanying drawing extracts the artwork of the novel process of sapogenin for a kind of yellow ginger of the present invention.
Five, concrete embodiment
Below in conjunction with embodiment the present invention is described in further detail:
1, take by weighing dried yellow ginger 1000Kg, coarse reduction is to 2-5mm
3, micro mist is broken to 400 orders again.
2, powder is dropped in the high-shear emulsifying jar, add aqueous ethanol or methyl alcohol, shear 30min.
3, the yellow ginger ultrasonication 60min after will shearing, separate solid particles gets alcohol solvent.
4, alcohol solvent distillation be concentrated into dried, the total saponin of residue.
5, total saponin adds the water suspendible, reject dissolving liquid glucose, and 80 ℃ of dryings of insolubles add 20% hydrochloric acid reacting by heating 4 hours.
6, filtering acid solution adds the neutralization of 1% yellow soda ash with the acidolysis precipitation, is washed to neutrality, and after drying gets the crude product sapogenin.
7, add anhydrous alcohol solution crude product sapogenin, and add the activated carbon powder heating for dissolving of total amount 1%.The filtering separation carbon dust, and with filter solvents after microporous membrane filters out impurities, reduction vaporization to flocks is separated out, the cooling solvent, 80 ℃ of evaporates to dryness behind the flocks suction strainer must be made with extra care 25 kilograms of sapogenins.
Claims (7)
1, a kind of new process of production of diosgenin, its technology is as follows:
(1), choosing 2-3 gives birth to yellow ginger or Ningpo Yam Rhizome collar (water ratio is less than 7%) and carries out coarse reduction and make its granularity reach 2-3mm
3, be crushed to 5-10um with supper micron mill again.
(2), in solid particles, cooperate reverse-flow ultrasonic circulating extracting machine to make cell wall breaking with 90-95% ethanol or methyl alcohol and handle; Filter and collect lixiviate filtrate, remove filter residue.Isolating pure liquid is done concentrated the distillation: A, alcohol solvent rectifying are reclaimed and are reused, and ethanol concentrated solution adding skim soln evaporated under reduced pressure gets total saponin; B, ethanol are concentrated into flocks and separate out, and after cold washing with alcohol flocks degreasing, 60-90 ℃ of heat drying gets yellow saponaceous solid.
(3), in the saponaceous solid of yellow, add immersions of purifying waste water, volume is 10 times of solid, is lower than 95 ℃ of heating with quickening immersion speed, filtrate liquid after 30 minutes is with insolubles 60-160 ℃ drying.
(4), dry thing adds 90-95% ethanol or methyl alcohol and is heated to dissolving fully; The canescence insoluble solids is separated out in cooling, and the micro-pore-film filtration reject is separated out impurity; 85-120 ℃ of heating concentrates reclaims pure liquid, and alcoholic solution concentrates to be cooled to separates out flocks fully, leaches pure liquid; 60-160 ℃ of drying separated out flocks and must be made with extra care saponin.
(5), refining saponin or total saponin heating for dissolving in the 15-35% hydrochloric acid soln, heating pyrolyze 4 hours becomes clear to liquid, hydrochloric acid solution and flocculent precipitate, leach acid solution.
(6), in flocculent precipitate with 1% yellow soda ash neutralization, be washed to neutrality, cryodrying, the crude product sapogenin.
(7), be aided with and be lower than 80 ℃ and be heated to after crude product sapogenin solid substance dissolves fully by adding ethanol in the crude product sapogenin, stop heating; Add activated carbon powder, pure liquid micro-pore-film filtration.
(8), reclaim alcoholic solution, 60-160 ℃ of cryodrying gets the elaboration sapogenin, or 80 ℃ of evaporating solvents directly the elaboration sapogenin.
2, according to the new process of production of the described a kind of diosgenin of claim 1, the new technology that it is applied to: (1) superfine communication technique; (2) high-shear technology; (3) reverse-flow ultrasonic circulating extractive technique; (4) screw settling isolation technique; (5) adopt the reciprocal lixiviate of chemical solvents; (6) membrane filtration technology; (7) electrodialysis technology.
3, the new process of production according to the described a kind of diosgenin of claim 1 is characterized in that adopting the cooperation of reverse-flow ultrasonic circulating extracting machine interpolation organic solvent that yellow ginger or Ningpo Yam Rhizome are made broken wall treatment.
4, the production new process of production of a kind of diosgenin according to claim 1 is characterized in that adopting ethanol or methanol solvate to cooperate extraction equipment Jin to propose aqueous saponin.
5, the new process of production of a kind of diosgenin according to claim 1 adopts the vacuum concentration distillating recovering solvent.
6, the new process of production of a kind of diosgenin according to claim 1, impurity and the pigment of its feature in adopting activated carbon pulvis adsorption solvent.
7, the new process of production of a kind of diosgenin according to claim 1 is characterized in that adopting micronizing equipment to carry out micronizing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510022745 CN1793162A (en) | 2005-12-28 | 2005-12-28 | Tech. for producing dioscorea sapogenin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510022745 CN1793162A (en) | 2005-12-28 | 2005-12-28 | Tech. for producing dioscorea sapogenin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1793162A true CN1793162A (en) | 2006-06-28 |
Family
ID=36804821
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510022745 Pending CN1793162A (en) | 2005-12-28 | 2005-12-28 | Tech. for producing dioscorea sapogenin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1793162A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101885750A (en) * | 2010-03-08 | 2010-11-17 | 李绍通 | Method for circularly processing and utilizing rhizome in dioscorea |
| CN101040696B (en) * | 2007-04-20 | 2011-09-21 | 瑞昌市渝瑞食品有限公司 | Processing technique of the integrated application of yam |
| CN102363801A (en) * | 2011-11-29 | 2012-02-29 | 周航 | Production process for diosgenin |
-
2005
- 2005-12-28 CN CN 200510022745 patent/CN1793162A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101040696B (en) * | 2007-04-20 | 2011-09-21 | 瑞昌市渝瑞食品有限公司 | Processing technique of the integrated application of yam |
| CN101885750A (en) * | 2010-03-08 | 2010-11-17 | 李绍通 | Method for circularly processing and utilizing rhizome in dioscorea |
| CN101885750B (en) * | 2010-03-08 | 2012-08-22 | 李绍通 | Method for circularly processing and utilizing rhizome in dioscorea |
| CN102363801A (en) * | 2011-11-29 | 2012-02-29 | 周航 | Production process for diosgenin |
| CN102363801B (en) * | 2011-11-29 | 2013-10-23 | 周航 | Production process for diosgenin |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102491938B (en) | A kind of purification process of S-GI | |
| CN101817853A (en) | Method for extracting tea saponin by adopting tea seed cake | |
| CN101182079B (en) | Citric acid mother liquor treatment process | |
| CN103204800B (en) | A kind of extracting method of 1 DNJ | |
| CN103936811A (en) | Tea seed meal superfine grinding and ultrasonic-assisted water-alcohol method for extraction of tea saponin | |
| CN102659910A (en) | High-efficiency extraction and cleaning production process for diosgenin | |
| CN1793162A (en) | Tech. for producing dioscorea sapogenin | |
| CN101560239B (en) | Production process for extracting saponin from yellow ginger by catalytic solvent method | |
| CN100460419C (en) | New cleanproduction process for extracting saponin from dioscorea zingiberensis | |
| CN102464700B (en) | Hydrolysis extraction process for yam diosgenin | |
| CN206828868U (en) | A kind of combination unit for separating cellulose, lignin and carbohydrate | |
| CN103641716A (en) | Method for extracting refined chicoric acid | |
| CN102660620A (en) | Method for extracting vernonia glycoside D | |
| CN1932022B (en) | Process of preparing high purity solanesol with potato leaf as material | |
| CN101885750B (en) | Method for circularly processing and utilizing rhizome in dioscorea | |
| CN1779070A (en) | Full component separation for cell wall of agricultural refuse | |
| CN108853299A (en) | A kind of extracting method of dragon's blood | |
| CN102336804A (en) | Method for extraction of diosgenin via steam explosion | |
| CN101709057B (en) | Extraction method of genistein | |
| CN102660655B (en) | Xylitol production technology | |
| CN1537865A (en) | Method of extracting lactoalbumin, nucleic acid oligosaccharide, isoflavone, saponin from yellow waste water generated by producing soybean | |
| CN101385750B (en) | Preparation method of effective ingredient of isatis root | |
| CN1325510C (en) | Method for producing dioscin by directly extracting saponin without pollution | |
| CN206219469U (en) | A kind of extraction extracts forulic acid device in wheat bran | |
| CN1768891A (en) | Extraction method and equipment of Chinese medicinal active component |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20060628 |